HCID 11379002、化合物 → HCID 178513055、化合物

HRID 898815ノート

反応式

HRID 898815 の反応式
C[O:2][C:3]([C:5]1[O:6][C:7]([C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][CH:11]=2)=[CH:8][CH:9]=1)=O.CS(O)(=O)=O.FC1C=CC=CC=1C1OC(C([NH:36][C:37]([NH2:39])=[NH:38])=O)=CC=1>CO.[Cl-].[Na+].O>[F:16][C:13]1[CH:14]=[CH:15][C:10]([C:7]2[O:6][C:5]([C:3]([NH:38][C:37]([NH2:39])=[NH:36])=[O:2])=[CH:9][CH:8]=2)=[CH:11][CH:12]=1

参加物

5

反応物 2

HCID 11379002HCID 11379002、化合物HCID 178505355HCID 178505355、化合物

生成物 1

HCID 178513055HCID 178513055、化合物収率 51.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

5-(4-fluorophenyl)furan-2-carboxylic acid methyl ester (220 mg, 1.0 mmol) was dissolved in methanol (4 ml), to which 2 M guanidine solution (3.0 ml, 6.0 mmol) prepared in Example 1 was added, and the mixture was heated at reflux for 12 hours. After completion of the reaction, the solution was added with saturated brine (20 ml) and extracted with ethyl acetate (30 ml×3). The organic layer was washed with 10% brine, dried over anhydrous magnesium sulfate (MgSO4), and concentrated in vacuo. The residue was purified by silica gel column chromatography (5% methanol/dichloromethane), to give 127 mg of a title compound (yield: 51%).

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux for 12 hours
  4. customAfter completion of the reaction
  5. extractionextracted with ethyl acetate (30 ml×3)
  6. washThe organic layer was washed with 10% brine
  7. dry with materialdried over anhydrous magnesium sulfate (MgSO4)
  8. concentrationconcentrated in vacuo
  9. customThe residue was purified by silica gel column chromatography (5% methanol/dichloromethane)

出典と根拠

ORDレコード
ord-df06d6e6b2ca4bd898935427db93b9e9
出典データセット
uspto-grants-2008_04
特許番号
US07351843B2

反応ノート

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